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通过快速共缩合法合成羧基修饰的棒状SBA-15

Synthesis of carboxyl-modified rod-like SBA-15 by rapid co-condensation.

作者信息

Shen Shoucang, Chow Pui Shan, Kim Sanggu, Zhu Kewu, Tan Reginald B H

机构信息

Institute of Chemical and Engineering Sciences, A*STAR (Agency for Science, Technology and Research), Jurong Island, Singapore.

出版信息

J Colloid Interface Sci. 2008 May 15;321(2):365-72. doi: 10.1016/j.jcis.2008.02.020. Epub 2008 Feb 19.

Abstract

Carboxyl-modified SBA-15 rod-like mesoporous materials have been synthesized by a facile rapid co-condensation of tetraethylorthosilicate (TEOS) and 2-cyanoethyltriethoxysilane (CTES), followed by hydrolysis of cyanide groups in sulfuric acid. The concentration of carboxylic groups was varied by changing the silica source ratio of CTES/TEOS from 0.05 to 0.3. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) showed that the uniform ordered mesoporous structure and rod-like morphology of SBA-15 have been preserved even at the high concentration of carboxylic groups employed. Characterization by Fourier transformed infrared spectroscopy (FTIR), solid-state NMR investigation indicated that carboxylic groups have been successfully grafted onto the surface of SBA-15 through siloxane bonds [(O(3))SiCH(2)CH(2)COOH. The negative charges of the modified SBA-15 materials were enhanced by the presence of the carboxylic groups on the surface. The capacity of lysozyme adsorption of the modified SBA-15 materials were found to be significantly improved as compared with pure silica SBA-15. The maximum amount of lysozyme adsorption on carboxyl-modified was increased with the pH of solution increased from 5.5 to 9.0.

摘要

通过正硅酸乙酯(TEOS)和2-氰基乙基三乙氧基硅烷(CTES)的简便快速共缩合,随后在硫酸中水解氰基,合成了羧基修饰的SBA-15棒状介孔材料。通过将CTES/TEOS的硅源比例从0.05改变到0.3来改变羧基的浓度。X射线衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)表明,即使在使用高浓度羧基的情况下,SBA-15的均匀有序介孔结构和棒状形态也得以保留。傅里叶变换红外光谱(FTIR)表征、固态NMR研究表明,羧基已通过硅氧烷键[(O(3))SiCH(2)CH(2)COOH成功接枝到SBA-15表面。表面羧基的存在增强了改性SBA-15材料的负电荷。发现与纯二氧化硅SBA-15相比,改性SBA-15材料的溶菌酶吸附能力显著提高。随着溶液pH从5.5增加到9.0,羧基修饰物上溶菌酶的最大吸附量增加。

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